Streamlined sample cleanup using combined dispersive solid-phase extraction and in-vial filtration for analysis of pesticides and environmental pollutants in shrimp |
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Authors: | Lijun Han Yelena Sapozhnikova Steven J. Lehotay |
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Affiliation: | 1. College of Science, China Agricultural University, Beijing, China;2. U.S. Dept. of Agriculture, Agricultural Research Service, Eastern Regional Research Center; 600 East Mermaid Lane, Wyndmoor, PA 19038, USA |
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Abstract: | A new method of sample preparation was developed and is reported for the first time. The approach combines in-vial filtration with dispersive solid-phase extraction (d-SPE) in a fast and convenient cleanup of QuEChERS (quick, easy, cheap, effective, rugged, and safe) extracts. The method was applied to simultaneous analysis of 42 diverse pesticides and 17 environmental contaminants, including polycyclic aromatic hydrocarbons, polychlorinated biphenyls (PCBs), and flame retardants, in shrimp as the sample matrix. Final extracts were analyzed by both low-pressure gas chromatography – triple quadrupole tandem mass spectrometry (LPGC-MS/MS), and high-performance liquid chromatography – triple quadrupole tandem mass spectrometry (HPLC-MS/MS) to provide a wide scope of analysis for targeted analytes. During method development, several different commercial sorbents for d-SPE were investigated and compared with respect to analyte recoveries. The method was validated at 10, 50, and 100 ng g−1 spiking levels (10-fold lower for PCBs), and the results for nearly all analytes were between 70 and 115% recoveries with ≤17% relative standard deviations. The method was shown to be simple, fast, and effective for multi-application analysis of chemical residues in the representative food and environmental marker matrix. |
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Keywords: | DPX, Disposable pipette extraction d-SPE, Dispersive solid-phase extraction FRs, Flame retardants HPLC-MS/MS, High-performance liquid chromatography &ndash tandem mass spectrometry IS, Internal standard LOD, Limit of detection LOQ, Limit of quantification LPGC-MS/MS, Low-pressure gas chromatography &ndash tandem mass spectrometry MRM, Multiple reaction monitoring PAHs, Polycyclic aromatic hydrocarbons PBBs, Polybrominated biphenyls PBDEs, Polybrominated diphenyl ethers PCBs, Polychlorinated biphenyls POPs, Persistent organic pollutants PSA, Primary secondary amine PVDF, Polyvinylidene fluoride QuEChERS, Quick, easy, cheap, effective, rugged, and safe TPP, Triphenylphosphate |
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